反应 #3587

反应方程式

10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine

2,4-dichlorobenzoyl chloride

triethylamine

→

desired product

收率 53.5%

N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-2,4-dichlorobenzamide

收率 53.5%

溶剂

ethyl acetate

methylene chloride

反应条件

后处理

1. 1
   其他The bath is removed
2. 2
   workup.STIRRINGthe reaction mixture stirred at room temperature for 18 hours
3. 3
   浓缩The volatiles are concentrated in vacuo
4. 4
   其他to give a residue which
5. 5
   洗涤washed with water, 2N citric acid, 1M NaHCO3 and brine
6. 6
   干燥The organic layer is dried with Na2SO4
7. 7
   过滤filtered
8. 8
   浓缩concentrated in vacuo
9. 9
   其他to give a residue which
10. 10
    其他is crystallized from ethyl acetate

实验过程

To a solution of 415 mg of 2,4-dichlorobenzoyl chloride in 5 ml of methylene chloride at 0° C. is added 346 μl of triethylamine. After stirring for 3 minutes, 500 mg of 10,11-dihydro-10-(4-aminobenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine is added. The bath is removed and the reaction mixture stirred at room temperature for 18 hours. The volatiles are concentrated in vacuo to give a residue which is dissolved in ethyl acetate, washed with water, 2N citric acid, 1M NaHCO3 and brine. The organic layer is dried with Na2SO4, filtered and concentrated in vacuo to give a residue which is crystallized from ethyl acetate to give 420 mg of the desired product as a crystalline solid, m.p., 210°-212° C.

来源